Effects of deposition parameters on laser-induced damage threshold of Ta2O5 films

Ta₂O₅ films were deposited on BK7 substrates by e-beam evaporation with different deposition parameters such as substrate temperature (323-623 K), oxygen pressure (0.5-3.0×10⁻² Pa) and deposition rate (0.2-0.5 nm/s). Absorption, scattering and chemical composition were investigated by surface thermal lensing (STL) technique, total integrated scattering (TIS) measurement and X-ray photoelectron spectroscopy (XPS), respectively. The laser-induced damage threshold (LIDT) was assessed using pulsed Nd:YAG 1064 nm laser at a pulse length of 12 ns. The results showed that optical properties, absorption and LIDT were influenced by the deposition parameters and annealing. However, scattering was little correlated with the deposition parameters. On the whole, the LIDT increased with increasing substrate temperature and oxygen pressure, whereas it increased firstly and then decreased upon increasing deposition rate. After annealing at 673 K for 12 h, the LIDT of films improved significantly. The dependence of possible damage mechanism on deposition parameters was discussed.     

Investigation of annealing effects on the laser-induced damage threshold of amorphous Ta2O5 films

Ta₂O₅ films were deposited using the conventional electron beam evaporation method and then annealed at temperatures in the range 373-673 K. Chemical composition, scattering and absorption were examined by X-ray photoelectron spectroscopy (XPS), total integrated scattering (TIS) measurement and the surface thermal lensing (STL) technique, respectively. The laser-induced damage threshold (LIDT) was assessed using the output from an Nd:YAG laser with a pulse length of 12 ns. The results showed that the improvement of the LIDT after annealing was due to the reduced substoichiometric and structural defects present in the film. The LIDT increased slightly below 573 K and then increased significantly with increase in annealing temperature, which could be attributed to different dominant defects. Moreover, the root mean square (RMS) roughness and scattering had little effect on the LIDT, while the absorption and the LIDT were in accord with a general relation.     

High temperature annealing effect on structure, optical property and laser-induced damage threshold of Ta2O5 films

Ta₂O₅ films were deposited by conventional electron beam evaporation method and then annealed in air at different temperature from 873 to 1273 K. It was found that the film structure changed from amorphous phase to hexagonal phase when annealed at 1073 K, then transformed to orthorhombic phase after annealed at 1273 K. The transmittance was improved after annealed at 873 K, and it decreased as the annealing temperature increased further. The total integrated scattering (TIS) tests and AFM results showed that both scattering and root mean square (RMS) roughness of films increased with the annealing temperature increasing. X-ray photoelectron spectroscopy (XPS) analysis showed that the film obtained better stoichiometry and the O/Ta ratio increased to 2.50 after annealing. It was found that the laser-induced damage threshold (LIDT) increased to the maximum when annealed at 873 K, while it decreased when the annealing temperature increased further. Detailed damaged models dominated by different parameters during annealing were discussed.     

Annealing effects on structure and laser-induced damage threshold of Ta2O5/SiO2 dielectric mirrors

The effects of annealing on structure and laser-induced damage threshold (LIDT) of Ta₂O₅/SiO₂ dielectric mirrors were investigated. Ta₂O₅/SiO₂ multilayer was prepared by ion beam sputtering (IBS), then annealed in air under the temperature from 100 to 400 °C. Microstructure of the samples was characterized by X-ray diffraction (XRD). Absorption of the multilayer was measured by surface thermal lensing (STL) technique. The laser-induced damage threshold was assessed using 1064 nm free pulsed laser at a pulse length of 220 μs.

It was found that the center wavelength shifted to long wavelength gradually as the annealing temperature increased, and kept its non-crystalline structure even after annealing. The absorbance of the reflectors decreased after annealing. A remarkable increase of the laser-induced damage threshold was found when the annealing temperature was above 250 °C.     

Influence of SiO2 additional layers on the laser induced damage threshold of Ta2O5 films

A series of Ta₂O₅ films with different SiO₂ additional layers including overcoat, undercoat and interlayer was prepared by electron beam evaporation under the same deposition process. Absorption of samples was measured using the surface thermal lensing (STL) technique. The electric field distributions of the samples were theoretical predicted using thin film design software (TFCalc). The laser induced damage threshold (LIDT) was assessed using an Nd:YAG laser operating at 1064 nm with a pulse length of 12 ns. It was found that SiO₂ additional layers resulted in a slight increase of the absorption, whereas they exerted little influence on the microdefects. The electric field distribution among the samples was unchanged by adding an SiO₂ overcoat and undercoat, yet was changed by adding an interlayer. SiO₂ undercoat. The interlayer improved the LIDT greatly, whereas the SiO₂ overcoat had little effect on the LIDT.     

Emission features of Ho ion in Nb2O5, Ta2O5 and La2O3 mixed Li2O-ZrO2-SiO2 glasses

Li₂O-ZrO₂-SiO₂: Ho³⁺ glasses mixed with three interesting d-block elemental oxides, viz., Nb₂O₅, Ta₂O₅ and La₂O₃, were prepared. Optical absorption and photoluminescence spectra of these glasses have been recorded at room temperature. The luminescence spectra of Nb₂O₅ and Ta₂O₅ mixed Li₂O-ZrO₂-SiO₂ glasses (free of Ho³⁺ ions) have also exhibited broad emission band in the blue region. This band is attributed to radiative recombination of self-trapped excitons (STEs) localized on substitutionally positioned octahedral Ta⁵⁺ and Nb⁵⁺ ions in the glass network. The Judd-Ofelt theory was successfully applied to characterize Ho³⁺ spectra of all the three glasses. From this theory various radiative properties, like transition probability A, branching ratio β_r and the radiative lifetime τ_r, for ⁵S₂ emission levels in the spectra of these glasses have been evaluated. The radiative lifetime for ⁵S₂ level of Ho³⁺ ions has also been measured and quantum efficiencies were estimated. Among the three glasses studied the La₂O₃ mixed glass exhibited the highest quantum efficiency. The reasons for such higher value have been discussed based on the relationship between the structural modifications taking place around the Ho³⁺ ions.     

Effects of annealing on laser-induced damage threshold of TiO2/SiO2 high reflectors

The mechanism of improving 1064 nm, 12 ns laser-induced damage threshold (LIDT) of TiO₂/SiO₂ high reflectors (HR) prepared by electronic beam evaporation from 5.1 to 13.1 J/cm² by thermal annealing is discussed. Through optical properties, structure and chemical composition analysis, it is found that the reduced atomic non-stoichiometric defects are the main reason of absorption decrease and LIDT rise after annealing. A remarkable increase of LIDT is found at 300 °C annealing. The refractive index and film inhomogeneity rise, physical thickness decrease, and film stress changes from compress stress to tensile stress due to the structure change during annealing.     

渐变折射率Ta2O5/SiO2薄膜多脉冲激光损伤特性

采用离子束溅射（IBS）的方式,制备了1064 nm高反射Ta2O5/SiO2渐变折射率光学薄膜。对其光学性能和在基频多脉冲下抗损伤性能进行了分析。 通过渐变折射率的设计方式,很好地抑制了边带波纹,增加了1064 nm反射率。通过对损伤阈值的分析发现,随着脉冲个数的增加,损伤阈值下降明显;但是在20个脉冲数后,损伤阈值（维持在22 J/cm2左右）几乎保持不变直到100个脉冲数。通过Leica显微镜对损伤形貌的观察,发现损伤诱因是薄膜表面的节瘤缺陷。通过扫描电镜（SEM）以及聚集离子束（FIB）对薄膜表面以及断面的观察,证实了薄膜的损伤起源于薄膜表面的节瘤缺陷。进一步研究得出,渐变折射率薄膜在基频光单脉冲下损伤主要是由初始节瘤缺陷引起的,在后续多脉冲激光辐照下初始节瘤缺陷引起烧蚀坑的面积扩大扫过薄膜上的其他节瘤缺陷,引起了其他节瘤缺陷的喷射使损伤加剧,造成损伤的累积效应。     

Structural and compositional changes in ion-bombarded Ta2O5

A detailed study of the effect of heavy-ion bombardment on Ta₂O₅ has been undertaken using a combination of radioactive tracer techniques, electron microscopy, and Rutherford backscattering. Crystalline Ta₂O₅ is amorphized at ~6 × 10¹³ ions cm^?2, while at a dose of ~5 × 10¹⁶ ions cm^?2 the electron microscopy reveals the development of random grains of a new crystalline phase. By ~1 × 10¹⁷ ions cm^?2 the grains are not yet overlapping but still yield a diffraction pattern consistent with either δ-Ta-O (not to be confused with TaO) or Ta_1?xO₂, thus indicating that Ta₂O₅, like most other transition-metal oxides, is subject to preferential sputtering. Preferential sputtering was confirmed by backscattering analysis of specimens bombarded to high doses, where the average surface composition was found to be Ta_1.8±0.2O₂ or, equivalently, Ta₂O_2.2±0.2. The surface alteration had an average composition independent of the mass and energy of the incident ions.     

Facile synthesis of Nb2O5 nanorod array films and their electrochemical properties

Nb₂O₅ nanorod array films were synthesized by a facile hydrothermal process using niobium metal foil and NH₄F as precursors. The Nb₂O₅ nanorods stand on the niobium metal foil substrate and are less than 100 nm in diameter and about 1 μm in length. X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM) characterizations indicate that these nanorods have orthorhombic structure and grew longitudinally along 〈0 0 1〉 direction. The nanorod growth mechanism was discussed. Thermal annealing at a temperature below 500 °C did not change the microstructure of nanorods but improve the crystallinity. The Nb₂O₅ nanorod array films have been tested as cathode material for lithium battery, which showed a good specific capacity up to 380 mAh g⁻¹ even after 50 charge/discharge cycles.     

渐变折射率Ta_2O_5/SiO_2薄膜多脉冲激光损伤特性

采用离子束溅射(IBS)的方式,制备了1064nm高反射Ta2O5/SiO2渐变折射率光学薄膜。对其光学性能和在基频多脉冲下抗损伤性能进行了分析。通过渐变折射率的设计方式,很好地抑制了边带波纹,增加了1064nm反射率。通过对损伤阈值的分析发现,随着脉冲个数的增加,损伤阈值下降明显;但是在20个脉冲数后,损伤阈值(维持在22J/cm2左右)几乎保持不变直到100个脉冲数。通过Leica显微镜对损伤形貌的观察,发现损伤诱因是薄膜表面的节瘤缺陷。通过扫描电镜(SEM)以及聚集离子束(FIB)对薄膜表面以及断面的观察,证实了薄膜的损伤起源于薄膜表面的节瘤缺陷。进一步研究得出,渐变折射率薄膜在基频光单脉冲下损伤主要是由初始节瘤缺陷引起的,在后续多脉冲激光辐照下初始节瘤缺陷引起烧蚀坑的面积扩大扫过薄膜上的其他节瘤缺陷,引起了其他节瘤缺陷的喷射使损伤加剧,造成损伤的"累积效应"。     

Temperature dependences of optical properties,chemical composition,structure,and laser damage in Ta2O5 films

Ta2O5 films are prepared by e-beam evaporation with varied deposition temperatures,annealing temperatures,and annealing times.The effects of temperature on the optical properties,chemical composition,structure,and laserinduced damage threshold(LIDT) are systematically investigated.The results show that the increase of deposition temperature decreases the film transmittance slightly,yet annealing below 923 K is beneficial for the transmittance.The XRD analysis reveals that the film is in the amorphous phase when annealed below 873 K and in thehexagonal phase when annealed at 1073 K.While an interesting near-crystalline phase is found when annealed at 923 K.The LIDT increases with the deposition temperature increasing,whereas it increases firstly and then decreases as the annealing temperature increases.In addition,the increase of the annealing time from 4 h to 12 h is favourable to improving the LIDT,which is mainly due to the improvement of the O/Ta ratio.The highest LIDT film is obtained when annealed at 923 K,owing to the lowest density of defect.     

Preparation and spectroscopic properties of Nb2O5 nanorods

Nb₂O₅ nanorods have been prepared using water/ethanol media. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-visible absorption and photoluminescence spectroscopy. The as-prepared Nb₂O₅ nanorods appeared to be single pseudohexagonal (TT-Nb₂O₅) phase. From the photoluminescence spectrum, two emission bands at 407 and 496 nm, respectively, were observed. The origin of the luminescence was discussed in detail.     

Waveguiding and photoluminescence in Er-doped Ta2O5 planar waveguides

The optimization of erbium-doped Ta₂O₅ thin film waveguides deposited by magnetron sputtering onto thermally oxidized silicon wafer is described. Optical constants of the film were determined by ellipsometry. For the slab waveguides, background losses below 0.4 dB/cm at 633 nm have been obtained before post-annealing. The samples, when pumped at 980 nm yielded a broad photoluminescence spectrum (FWHM∼50 nm) centred at 1534 nm, corresponding to ⁴I_13/2-⁴I_15/2 transition of Er³⁺ ion. The samples were annealed up to 600 °C and both photoluminescence power and fluorescence lifetime increase with post-annealing temperature and a fluorescence lifetime of 2.4 ms was achieved, yielding promising results for compact waveguide amplifiers.     

Fabrication of three-dimensionally ordered macroporous Ta2O5 films through aqueous organic gel process

Ta₂O₅ thin films have been prepared in the forms of three-dimensionally ordered macroporous (3-DOM) materials through aqueous organic gel process guided by polystyrene (PS) colloidal templates. The structure of the films was strongly affected by the infiltration process. This suggests that the infiltration process which aims at introducing desired materials into the interstitial spaces between the PS templates is of critical importance. Dip-drawing method was adopted for infiltration in this article. However, excess precursor worked as a capping agent for films prepared from the precursor of high concentration. Spin-coating method can efficiently remove the excess precursor by high speed rotating, which makes it a promising process for the infiltration of Ta-citric precursor with concentration higher than 0.5 mol/L. X-ray diffraction (XRD) pattern showed that the products can crystallize at 600 °C and had a pure orthorhombic phase. The chemical composition of the product was also studied by X-ray photoelectron spectroscopy (XPS).     

Composition of Ta2O5 stacked films on N2O- and NH3-nitrided Si

The composition and microstructure of rf sputtered 20 nm Ta₂O₅ on N₂O or NH₃ Rapid Thermal Nitrided (RTN) Si substrates have been investigated by X-ray photoelectron spectroscopy. RTN at 800 and 850 °C is effective to suppress active oxidation of Si. There is no evidence for the presence of SiO₂ at Si interface. A lightly nitrided surface is established in both cases without a formation of detectable oxynitride layer at Si. A layered nature of the films is observed, with stoichiometric tantalum pentoxide at and close to the films’ surface. In the depth, the films are mixed ones whose composition depends on the nitridation ambient. N₂O treatment stimulates oxidation processes during the film deposition while NH₃ nitridation results to a less effective oxidation and produces Ta-silicate like film. The correlation between the composition of the interfacial regions and the nitridation gas is also discussed. The results suggest that hydrogen, as a component of nitridation ambient, plays significant role in the reactions controlling the exact composition of the deposited Ta₂O₅, activating reactions with nitrogen. Nitrogen related reactions likely occur with NH₃ processing but do not with N₂O one. The presence of nitrogen feature is not detected in N₂O-samples spectra at all. In the integration perspective, preliminary RTN of Si in N₂O or NH₃ could be a suitable way to produce layered Ta₂O₅-based films with more or less presence of tantalum silicate with a trace of nitrogen, either only at the interface with Si (N₂O-process) or in the whole film (NH₃-process).     

金属醇盐法制备Ta2O5气凝胶

以乙醇钽为前驱物,采用金属醇盐溶胶-凝胶技术,获得了Ta2O5湿凝胶,分析了不同条件下的溶胶-凝胶过程,并初步探讨了凝胶过程机理。Ta2O5的溶胶-凝胶过程主要受到水量、催化剂用量及钽源浓度等因素的影响：体系在强酸性条件下凝胶,且随着酸性的增强,体系凝胶时间明显缩短;当水量较少时,凝胶时间随水量的增加而增加,但当水量增加到一定程度时,体系凝胶时间基本不变;实验证明,通过增大溶剂用量,体系凝胶时间延长,气凝胶理论密度降低。通过对溶胶-凝胶过程的控制,结合超临界干燥技术,获得了密度低至44 mg/cm3的Ta2O5气凝胶样品。     

Influence of overcoat on laser-induced damage threshold of 532 and 800 nm TiO2/SiO2 high reflectors

TiO₂/SiO₂ high reflectors with and without a SiO₂ overcoat are deposited by electron-beam evaporation. The film properties are characterized by visible spectrometry measures, structure analysis, roughness and laser-induced damage threshold (LIDT) tests, surface defects and damage morphology observation. The effects of overcoats on LIDT at 532 nm, 8 ns and 800 nm, 220 ps laser pulses are investigated. The relations between film structure, roughness, surface defects, electric field and LIDT are discussed. It is found that overcoats can increase the LIDT at these two laser wavelengths. The reduction of peak temperature, the low defects density and roughness, the low intrinsic absorption of SiO₂ and its amorphous structure are the main reasons for LIDT improvement by overcoats.     

Ta2O5/Ta界面分析的新模型

对Ta₂O₅/Ta样品界面区的深度剖面曲线进行了研究。基于离子溅射引起影响层存在的考虑,提出一种解释该曲线的新模型。通过此模型能很好地拟合实验曲线,并反映了溅射过程中的离子混合效应、原子堆积效应及相应的特征参数。样品由阳极氧化法制得,其厚度为500埃。表面分析在PHI-590型扫描俄歇微探针上完成,所有测量均在室温下进行。研究表明:深度剖面曲线并不符合误差函数分布;影响层的厚度为30—50埃,它是进行深度剖面分析时,决定元素俄歇信号强度的第一位重要因素;深度剖面 关键词：